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1.
The results of DSC studies of NaBH4–KBF4 mixtures are presented. It is shown by chemical analysis, XRD analysis, IR spectroscopy, and 11B and 9F MAS NMR that the decomposition of the mixtures starts at ~563 K to yield polyhedral borohydride compounds (predominantly B12H122-) in the solid residue. This temperature is much lower than the decomposition temperature of pure NaBH4 (749 K). The mechanism of formation of the B12H122- anion has been proposed and confirmed. According to this mechanism, boron atoms from KBF4 are involved in the formation of this anion.  相似文献   

2.
A new post-chemiluminescence (PCL) phenomenon was observed when phenothiazine medications were injected into the reaction mixture after the chemiluminescence (CL) reaction of luminol and potassium ferricyanide had finished. A possible reaction mechanism was proposed based on studies of the kinetic characteristics of the CL, CL spectra, fluorescence spectra, and on other experiments. The feasibility of determining various phenothiazine medications by utilizing these PCL reactions was examined. A molecular imprinting–post-chemiluminescence (MI-PCL) method was established for the determination of chlorpromazine hydrochloride using a chlorpromazine hydrochloride-imprinted polymer (MIP) as the recognition material. The method displayed high selectivity and high sensitivity. The linear range of the method was 1.0×10−8∼1.0×10−6, with a linear correlation coefficient of 0.9985. The detection limit was 3×10−9 g/ml chlorpromazine hydrochloride, and the relative standard deviation for a 1.0×10−7 g/ml chlorpromazine hydrochloride solution was 4.0% (n=11). The method has been applied to the determination of chlorpromazine hydrochloride in urine and animal drinking water with satisfactory results.   相似文献   

3.
The kinetics of the formation of iron carbides during the activation of iron-coated catalyst for Fischer–Tropsch synthesis promoted by copper and potassium, and by carbon monoxide and syngas, is studied. It is established that the presence of copper lowers the initial temperature of hematite reduction to magnetite and leads to the formation of carbide in both CO and СО/Н2. Potassium slows the rate of magnetite formation, but it accelerates the formation of iron oxide. It is shown that the rate of carbide formation during magnetite reduction for catalysts is half that in the reaction of hematite reduction to magnetite in both CO and СО/Н2.  相似文献   

4.
A simple and highly efficient protocol has been developed for the Pd/C-catalyzed ligand-free Suzuki–Miyaura reaction of potassium aryltrifluoroborates. In this catalytic system, the results demonstrate that oxygen plays a positive role in the cross-coupling reaction. In addition, this catalytic system could be successfully applied to synthesize biaryl compounds containing a carbazole moiety and the catalyst was recycled seven times without significant loss of catalytic activity.  相似文献   

5.
The effect of potassium and calcium additives on the catalytic activity of the Ce0.8Zr0.2O2 system in the reaction of CO oxidation was studied. With the use of X-ray diffraction analysis, it was found that the Ce0.8Zr0.2O2 and Ce0.8Zr0.2O2–Ca,K samples contained a mixed oxide of cerium and zirconium; the presence of the independent phases of potassium and calcium compounds in the modified system was not detected. With the use of the low-temperature adsorption–desorption of nitrogen, X-ray photoelectron spectroscopy, and temperature-programmed reduction, it was established that the Ce0.8Zr0.2O2–Ca,K system (in spite of the fact that its specific surface area was lower than that of Ce0.8Zr0.2O2) contained more active oxygen on the surface; peroxide and superoxide complexes formed upon the chemisorption of O2 can act as active oxygen species. This can be the reason for a higher efficiency of the Ce0.8Zr0.2O2–Ca,K system in comparison with that of the unmodified oxide. The results obtained indicate that the ash impurities of Ca and K can increase the catalytic activity of the biomorphic mixed oxides Ce0.8Zr0.2O2 prepared with the use of sawdust as a template.  相似文献   

6.
Potassium tantalate (KT) thin films and powders of both K2Ta2O6 (KT pyrochlore) and KTaO3 (KT perovskite) structures were prepared by means of chemical solution deposition method using Si(111) with ZnO and MgO buffer layers as a substrate. The influence of reaction atmosphere on reaction pathway and phase composition for both KT powders, and KT thin films has been studied mainly by means of powder diffraction and infrared spectroscopy. When an oxygen flow instead of static air atmosphere has been used the process of pyrolysis in oxygen runs over much narrower temperature interval (200–300 °C), relatively to air atmosphere (200–600 °C) and almost no (in case of powders), or no (in case of thin films) pyrochlore intermediate phase has been detected in comparison with treatment in air, where the pyrochlore phase is stable at temperatures 500–600 °C (powders). KT perovskite phase starts to crystallize at temperatures 50° and 150 °C lower compared to air atmosphere in case of powders and thin films, respectively. Microstructure formed by near-columnar grains and small grains of equiaxed shape was observed in films treated in oxygen and air atmosphere, respectively.  相似文献   

7.
8.
The six-membered phosphorinane ring in (1,4,7,10,13,16-hexaoxa­cyclo­octa­decane)­potassium 2-O-benzoyl-1,3,5-O-methyl­idyne-myo-in­osi­tol 4,6-cyclo­phosphate trihydrate, [K(C12H24O6)](C14H12O9P)·3H2O, has a boat rather than a chair conformation. The K+ ion is eight-coordinate and is connected to one of the phosphate O atoms, one of the O atoms of the myo-inositol residue and the six O atoms of the crown ether.  相似文献   

9.
Experimental data on the sol–gel synthesis of manganese oxides formed during the reduction of potassium permanganate by polyvinyl alcohol in an aqueous medium are presented. The physicochemical properties of the obtained manganese oxide systems that depend on the conditions of the synthesis are studied by means of DTA, XRD, SEM, and the low temperature adsorption–desorption of nitrogen. It is found that the obtained samples have a mesoporous structure and predominantly consist of double potassium–manganese oxide K2Mn4O8 with a tunnel structure and impurities of oxides such as α-MnO2, MnO, α-Mn2O3, and Mn5O8. It is shown that the proposed method of synthesis allows us to regulate the size and volume of mesopores and, to a lesser extent, the texture of the obtained oxides, which can be considered promising sorbents for the selective extraction of strontium and cesium ions from multicomponent aqueous solutions.  相似文献   

10.
The effect of potassium(K) promoter on the catalytic performance of activated carbon(AC) supported Wacker-type catalysts(Pd Cl2–Cu Cl2/AC) for the synthesis of dimethyl carbonate(DMC) from CO and methyl nitrite(MN) was investigated by means of N2 adsorption, H2-temperature-programmed reduction(H2-TPR), and X-ray photoelectron spectroscopy(XPS). The experimental results showed that the space time yield of DMC on Wacker-type catalysts with different K promoters ranked in the following order: KCl KOH CH3 COOK K2CO3. Especially, the addition of KCl significantly improved the catalytic activities of Pd Cl2–Cu Cl2/AC catalyst for DMC synthesis from CO and MN. N2 adsorption data indicated that the addition of K promoters did not change the textural properties of Wacker-type catalysts greatly. H2-TPR and XPS results demonstrated that the existence of KCl promoted the reducibility of Cu2+species and increased the proportion of Cu2+species on catalyst surface, which is favorable for oxidizing Pd0 to active Pd2+. Further, the addition of KCl benefited the reactivity of Pd Cl2–Cu Cl2/AC catalyst for DMC synthesis from CO and MN.  相似文献   

11.
Thermal studies, sometimes together with X-ray analysis, were applied to investigate the process of hydration in the systems calcium silicates (tricalcium silicate or dicalcium silicate) - water - electrolyte. Alkali metal or alkaline-earth metal salts were used as electrolytes. Results and conclusions are presented concerning the action of electrolytes upon the kinetics of hardening of the calcium silicates and the composition and phase transformation of calcium hydrosilicate in the presence of low proportions of electrolytes (0.5, 2 and 5 mass%), these effects being due to ionic substitution. A higher proportion of electrolyte (above 2%) in the systems calcium silicate-water can determine the formation of a complex salt, e.g. calcium hydroxysalts or double hydrosilicates. This revised version was published online in August 2006 with corrections to the Cover Date.  相似文献   

12.
Treatment of potassium bromodifluoroacetate(1)with alkyl halides in thepresence of copper,iodide and potassium fluoride in DMF at 85—90℃ for 3—5h gavethetrifluoromethylated derivatives in moderate to high yields.  相似文献   

13.
Kinetic analysis of the crystallization process in Bi4(As2S3)96 and Bi6(As2S3)94 glasses was performed based on DSC curves recorded under non-isothermal measurement conditions. Samples were thermally treated at different heating rates in the temperature range 300?C770?K. The activation energy of crystallization E and the pre-exponential factor K 0 are determined by the Kissinger method and the characteristic crystallization parameters m and n of investigated glasses by the Matusita method. For both crystallization processes the glass with 4 at.% of Bi is characterized by the mechanism of volume nucleation, which is manifested in the form of two-dimensional growth at the first crystallization process, and as three-dimensional at the second one. On the other hand, in the sample with 6 at.% Bi, the average value of the parameter m is close to one, which indicates one-dimensional crystal growth. Compatibility of the values of the parameters m and n suggests that this sample has a large number of crystallization centers, which do not increase significantly during the thermal treatment.  相似文献   

14.
《Fluid Phase Equilibria》1999,164(2):267-273
Liquid–liquid equilibrium data for the ternary system 1-pentanol–ethanol–water have been determined experimentally at 25, 50, 85 and 95°C. These results have been correlated simultaneously by the uniquac method obtaining two sets of interaction parameters: one of them independent of the temperature and the other with a linear dependence. Both sets of parameters fit the experimental results well.  相似文献   

15.
In China the roots of Euphorbia kansui T.N. Liou ex T.P. Wang, known as ‘kansui’, have been used for centuries as a herbal remedy for edema, ascites, and asthma. Kansui, has inflammatory and tumor-promoting toxicity, and other side-effects, however, which have seriously restricted its clinical application. In the work discussed in this paper a simple and rapid LC–DAD–ESI-MS–MS method has been established for separation and characterization of the main compounds in the toxic fraction of E. kansui roots. Twelve diterpene derivatives were identified in the inflammatory fraction of kansui: kansuinine C, kansuinine B, kansuinine A, kansuinine D, 5-O-benzoyl-20-deoxyingenol, kansuinine E, kansuiphorin C, 3-O-benzoyl-20-deoxyingenol, 3-O-(2′E,4′Z-decadienoyl)-5-O-acetylingenol, 3-O-(2′E,4′Z-decadienoyl)-20-deoxyingenol, 20-O-(2′E, 4′E-decadienoyl)ingenol, and 3-O-(2′E,4′Z-decadienoyl)-20-O-acetylingenol. The inflammatory fraction was separated on a C18 reversed-phase column with a mobile phase gradient. The proposed method is a scientific and technical platform enabling the herbal medicine industry to perform quality control and ensure the safety of preparations that contain this class of poisonous diterpenoids.  相似文献   

16.
The effect of the acid–base properties of zeolite Y on the activity of palladium–zeolite catalysts for CO oxidation was studied. The modification of the support with basic additives was found to improve the catalyst activity. A linear correlation between the ratio between the amounts of O2and CO adsorbed on the surface of palladium and the catalyst activity was established.  相似文献   

17.

Abstract  

Supported iron catalysts are active for hydrocarbon oxidation with H2O2, but the hydrogen peroxide dismutation is a shortcoming that may constrain their applications. Herein, we attempted to address this problem using potassium and phosphate-doped iron oxide–silica nanocomposite (KPFeSi) synthesized via sol–gel methods. The promoted silica–iron oxide nanocomposite has been characterized by elemental analyses, FTIR, X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) surface-size determination. The synthesized KPFeSi was an active catalyst in the low-temperature liquid phase oxidation of various alkyl aromatics with hydrogen peroxide in conversions of 31–78%. Furthermore, the direct oxidation of benzene into phenol using hydrogen peroxide has been achieved in the absence of any acid with this KPFeSi compound.  相似文献   

18.
Journal of Radioanalytical and Nuclear Chemistry - A new MOFs-based adsorbent UiO-66@iPCC5 was prepared by hybridization of 25,27-bis(iso-propoxyl)-calix[4]arene-26,28-crown-5 (iPCC5) into the...  相似文献   

19.
Summary The amide conformers of two compounds and their enantiomers have been separated by liquid chromatography on an 1-acid glycoprotein column. The effects of organic modifier and pH on the separations obtained were investigated. The conformers of one of the compounds were separated micro-preparatively at low temperature on the same column using a D2O-based eluent; D2O had no deleterious effects on the chromatography obtained. Some preliminary competition experiments on one of the amides and a close analogue are presented.  相似文献   

20.
The kinetic of deuteration of -phenylpropionic acid with D2O acidified with HCl in the presence of homogeneous K2PtCl4 catalyst has been investigated in the 100–130°C temperature interval. The quasi-unimolecular H/D exchange rate constants at 100 and at 130°C, corresponding to fast H/D exchange process, have been deduced by analysis of the composite integrated NMR signal of the substituted benzene ring hydrogens; the Arrhenius activation energy for this exchange was estimated.  相似文献   

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